Preparation of lubricating compositions



Patented Aug. 7, 1951 'assams PREPARATION OF LUBRICATING COMPO SITIONS Marshall Duke, Summit, N. J Joseph Rio, Cumberland, Md., and Conrad Hohing, Jr., Morristown, N. J., assignors to Celanese Corporation of America, New York, N. Y., a corporation of Delaware No Drawing. Application November 26, 1949, Serial No. 129,792

9 Claims. (01. 252-837) This invention relates to lubricating compositions and relates more particularly to a process for preparing lubricating compositions containing dehydrated and desalted sulfonated fatty materials.

Many of the compositions that are employed at the present time for lubricating textile materials such as yarns, filaments, fibers and the like contain as essential ingredients a water-immiscible lubricant such as mineral, animal and/or vegetable oil, and the like in admixture with one or more dehydrated and desalted sulfonated fatty materials such as, for example, sulfonated an.i mal and vegetable oils and fats, and sulfonated long chain fatty acids and the esters thereof. For example, a satisfactory lubricating composition for cellulose acetate and other organic derivative of cellulose textile materials may be prepared by blending into a mineral oil a dehydrated and desalted sulfonated mixture of a mineral oil, a vegetable oil, and a long chain fatty acid, which mixture also includes an alkyl phenol to stabilize the same and to act as a penetrant and an antioxidant.

In preparing this lubricating composition, it has hitherto been the practice to remove the Water and inorganic salts that are formed during the preparation of the sulfonated fatty materials, by adding thereto anhydrous isopropyl alcohol in an amount sufficient to cause all of said inorganic salts to precipitate. The precipitated, salts are filtered out and the isopropyl alcohol distilled off, the water which is present in the sulfonated fatty materials coming off as an azeotrope with the isopropyl alcohol. water remains, a further quantity of anhydrous isopropyl alcohol is added and the mixture again distilled to remove the remaining water as well as the alcohol. The dehydrated and desalted sulfonated fatty maetrials are then blended with a mineral oil, producing a textile lubricating composition that is particularly suited for cellulose acetate and other organic derivative of cellulose textile materials.

Because of the many steps involved in their preparation, the dehydrated and desalted sulfonated fatty materials obtained by the process described above are expensive. Moreover, their properties vary considerably, often falling outside a commercially acceptable range; accordingly these dehydrated and desalted sulfonated fatty materials are frequently not suited for the production of lubricating compositions and must be discarded, A further expense involved in preparing these dehydrated and desalted sulfonated If any,

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fatty materials is the necessity for drying the wet isopropyl alcohol that is distilled therefrom to put the alcohol in condition for further use.

It is an important object of this invention to provide a novel process for preparing lubricating compositions containing dehydrated and desalted sulfonated fatty materials which will be free from the foregoing and other disadvantages of the processes hitherto employed for this purpose and which will be especially efiicient and inexpensive.

A further object of this invention is the provision of a process for the preparation of lubricating compositions containing dehydrated and desalted sulfonated fatty materials which will require a minimum number of steps and which will yield products having consistently uniform properties.

Other objects of this invention will be apparent from the following detailed description and claims.

We have now discovered that the treatment of the sulfonated fatty materials with anhydrous isopropyl alcohol followed by filtration and distillation may be eliminated by combining the dehydration and desalting of the sulfonated fatty ,materials with the blending of said sulfonated fattymaterials into the lubricating composition. In accordance with our invention, sulfonated fatty materials containing water and inorganic salts such as, for example, the materials obtained by the neutralization with an alkaline material of a sulfonation reaction mixture, are distilled under subatmospheric pressure until all or substantially all of the water is eliminated therefrom. Then, the sulfonated fatty materials are blended with the lubricant that is to be present in the lubricating composition, whereupon the inorganic salts that are contained in the sulio nated fatty materials are precipitated owing to their insolubility in the lubricating composition so formed, The precipitated salts are then separated and the resulting lubricating composition is ready for use without further treatment. By carrying out the preparation of lubricating compositions containing dehydrated and desalted sulfonated fatty materials in this manner, the

total number of steps and the time required for this preparation is reduced by more than onehalf and, in addition, the products obtained are .more consistently uniform in their properties.

In carrying out the process of our invention a mixture of about 290 to 880 parts by weight of a mineral oil, about to 325 parts by weight of a vegetable oil such as, for example, rice oil,

olive oil, or peanut oil and about 220 to 670 parts by Weight of a long chain fatty acid such as, for example, oleic acid is sulfonated by treatment with fuming sulfuric acid such as, for example, 20% oleum at a temperature no greater than about 20 C. From about 50 to 160 parts of an alkyl phenol such as, for example, diamyl phenol is added to the sulfonation mixture, following which the free sulfuric acid in the sulfonation mixture is neutralized by the addition thereto of an aqueous solution of an alkaline material such as, for example, sodium hydroxide or potassium hydroxide. The neutralized sulfonation mixture is distilled under subatmospheric pressure, say less than about 50 mm. of mercury, at a temperature below that at which the sulfonated materials decompose. For example, when the distillation is carried out at a pressure of about 3040 mm. of mercury, the temperature should be maintained below about 70 C. After all or substantially all of the water is distilled from the sulfonation mixture, the sulfonated fatty materials are blended with about 1500 to 3000 parts by weight of a. mineral oil. The inorganic salts precipitate out and may be readily separated from the lubricating composition by filtration, for example. Prior to the filtration, a filter aid such as diatomaceous earth, bentonite and the like may be added to the lubricating composition to improve the eiiiciency of filtration and the clarity of the filtrate.

The following example is given to illustrate this invention further.

Example tained at a temperature of C. there is added over a period of 30 minutes 135 parts by weight of 20% oleum. The mixture is raised in a period of minutes to a temperature of C.

The mixture is stirred vigorously for 45 minutes while maintaining the temperature between 19 and 21 C. To the sulfonated materials there is added 105 parts by weight of diamyl phenol, following which the free sulfuric acid in the mixture is neutralized by the addition of 187.5 parts by weight of a 50% by weight aqueous sodium hydroxide solution with vigorous stirring and artificial cooling to return the mixture to room temperature as rapidly as possible.

A charge of 500 parts by weight of the neutralized sulfonated materials is entered into a vessel equipped with a stirrer and the pressure in said vessel reduced to between and mm. of mercury. The temperature is raised gradually with stirring to 70 C. and held at this point until no more water distills off.

To 38 parts by weight of the dehydrated sulfonated materials there is added with stirring 62 parts by weight of a mineral oil having a viscosity of 50 (SUV) at 100 F. and 1 part by weight of diatomaceous earth and the mixture stirred vigorously for one hour. The mixture is filtered through a bed of diatomaceous earth to yield a sparkling clear lubricating composition which has a water content of 0.24% and an inorganic salt content of 0.01% and may be used without further treatment for lubricating cellulose acetate and other organic derivative of cellulose textile materials.

It is to be understood that the foregoing detailed description is given merely by way of illus- 4 tration and that many variations may be made therein without departing from the spirit of our invention.

Having described our invention, what we de sire to secure by Letters Patent is:

1. In a process for preparing lubricating com positions containin a lubricant selected from the class consisting of mineral, animal and vegetable oils and dehydrated and desalted sulfonated fatty materials from sulfonated fatty materials containing water and inorganic salts, the steps which comprise distilling the water from the sulfonated fatty materials, blending the dehydrated sulfonated fatty materials with the lubricant whereby the inorganic salts are precipitated, and separating the inorganic salts from the lubricating composition so formed.

2. In a process for preparing lubricating compositions containing a lubricant selected from the class consisting of mineral, animal and vegetable oils and dehydrated and desalted sulfonated fatty materials from sulfonated fatt materials con tainin water and inorganic salts, the steps which comprise distilling the water from the sulfonated fatty materials at subatmospheric pressure,

blending the dehydrated sulfonated fatty materials With the lubricant whereby the inorganic salts are precipitated, and separating the mor ganic salts from the lubricatin' composition so formed.

3. In a process for preparing lubricating compositions containing a lubricant selected from the class consisting of mineral, animal and vegetable oils and dehydrated and desalted sulfonated fatty materials from sulfonated fatty materials containing water and inorganic salts, the steps which comprise distilling the water from the sulfonated fatty materials at a subatmospheric pressure of less than about 50 mm. of mercury, blending the dehydrated sulfonated fatty materials with the lubricant whereby the inorganic salts are precipitated, and separating the inorganic salts from the lubricating composition so formed.

4. In a process for preparing lubricating compositions containing a mineral oil and a dehydrated and desalted sulfonated mixture of a mineral oil, a vegetable oil and a long chain fatty acid from a sulfonated mixture of a mineral oil, a vegetable oil and a long chain fatty acid con taining water and inorganic salts, the steps which comprise distillin the Water from the sulfonated mixture of a mineral oil, a vegetable oil and a long chain fatty acid, blending the dehydrated sulfonated mixture of a mineral oil, a vegetable oil and a long chain fatty acid with the mineral oil whereby the inorganic salts are precipitated, and separating the inorganic salts from the lubricating composition so formed.

5. In a process for preparing lubricating compositions containing a mineral oil and a dehydrated and desalted sulfonated mixture of a mineral oil, a'vegetable oil and a long chain fatty acid from a sulfonated mixture of a mineral oil, a vegetable oil and a long chain fatty acid containing water and inorganic salts, the steps which comprise distilling the water from the sulfonated mixture of a mineral oil, a vegetable oil and a long chain fatty acid at a pressure below about 50 mm. of mercury and at a temperature below about 70 C., blendin the dehydrated sulfonated mixture of a mineral oil, a vegetable oil and a long chain fatty acid with the mineral oil whereby the inorganic salts are precipitated, and separating the inorganic salts from the lubricating composition so formed.

6. In a process for preparing lubricating compositions containing a mineral oil and a dehydrated and desalted sulfonated mixture of a mineral oil, a vegetable oil and a long chain fatty acid from a sulfonated mixture of a mineral oil, a vegetable oil and a long chain fatty acid containing water and inorganic salts, the steps which comprise distilling the water from a sulfonated mixture of about 290 to 880 parts by weight of a mineral oil, about 105 to 325 parts by weight of a vegetable oil and about 220 to 670 parts by weight of a long chain fatty acid at subatmospheric pressure, blending the dehydrated sulfonated mixture of a mineral oil, a vegetable oil and a long chain fatty acid with about 1500 to 3000 parts by weight of a mineral oil whereby the inorganic salts are precipitated, and separating the inorganic salts from the lubricating composition so formed.

'7. In a process for preparing lubricating compositions containing a mineral oil and a dehydrated and desalted sulfonated mixture of a mineral oil, peanut oil and oleic acid from a sulfonated mixture of a mineral oil, peanut oil and oleic acid containing water and inorganic salts, the steps which comprise distilling the water from a sulfonated mixture of about 290 to 880 parts by weight of mineral oil, about 105 to 325 parts by weight of peanut oil and about 220 to 6'70 parts by weight of oleic acid at a subatmospheric pressure of less than about 50 mm. of mercury and at a temperature below about 70 (3., blending the dehydrated sulfonated mixture of mineral oil, peanut oil and oleic acid with from 150-0 to 3000 parts by weight of mineral oil whereby the inorganic salts are precipitated, and separating the inorganic salts from the lubricating composition so formed.

8. In a process for preparing lubricating compositions containing a mineral oil and a dehydrated and desalted sulfonated mixture of a mineral oil, peanut oil and oleic acid from a sulfonated mixture of a mineral oil, peanut oil and oleic acid containing water and inorganic salts, the steps which comprise distilling the water from a sulfonated mixture of 585 parts by weight of mineral oil, 215 parts by weight of peanut oil and 445 parts by weight of oleic acid at a subatmospheric pressure of 30 to 40 mm. of mercury and at a temperature of C., blending 38 parts by weight of the dehydrated sulfonated mixture of mineral oil, peanut oil and oleic acid with 62 parts by weight of mineral oil whereby the inorganic salts are precipitated, and separating the inorganic salts from the lubricatin composition so formed.

9. In a process fOr preparing lubricating compositions containing a lubricant selected from the class consisting of mineral, animal and vegetable oils and dehydrated and desalted sulfonated fatty materials selected from the class consisting of sulfonated animal and vegetable oils and fats, and sulfonated long chain fatty acids and the esters thereof from sulfonated fatty materials containing water and inorganic salts, the steps which comprise distilling th water from the sulfonated fatty materials, blending the dehydrated sulfonated fatty materials with the lubricant whereby the inorganic salts are precipitated, and separating the inorganic salts from the lubricating composition so formed.

MARSHALL DUKE. JOSEPH RIO. CONRAD HOHING, JR.

REFERENCES CITED The following references are of record in the file of this patent:

UNITED STATES PATENTS Number Name Date 2,406,408 Seymour et a1 Aug. 27, 1946 2,479,644 Seymour et a1 Aug. 23, 1949 

1. IN A PROCESS FOR PREPARING LUBRICATING COMPOSITIONS CONTAINING A LUBRICANT SELECTED FROM THE CLASS CONSISTING OF MINERAL, ANIMAL AND VEGETABLE OILS AND DEHYDRATED AND DESALTED SULFONATED FATTY MATERIALS FROM SULFONATED FATTY MATERIALS CONTAINING WATER AND INORGANIC SALTS, THE STEPS WHICH COMPRISE DISTILLING THE WATER FROM THE SULFONATED FATTY MINERALS, BLENDING THE DEHYDRATED SULFONATED FATTY MINERALS WITH THE LUBRICATING WHEREBY THE INORGANIC SALTS ARE PRECIPITATED, AND SEPARATING THE INORGANIC SALTS FROM THE LUBRICATING COMPOSITION SO FORMED. 